Ultrafine particles of ferromagnetic nanocrystalline Ni was synthesized by a novel chemical method in aqueous medium. Compositional analysis by Energy dispersive X–ray analysis showed that the as-prepared Ni powders are pure. Crystalline size of as-prepared Ni Powders was controlled by precursor concentration. X-ray diffraction studies indicated fcc crystal structure. Saturation magnetization increases as a function of crystalline size. Surface morphologies and magnetic properties were discussed.